Apparatus and method for continuous lyophilization
View Patent ↗A method and apparatus for the continuous sublimation of a substance includes cascading a material containing a substance capable of sublimation, such as water, between a plurality of trays vertically stacked within a processing zone provided within a processing chamber. A substantially atmospheric environment is maintained within the processing zone at a temperature whereby the substance sublimes forming a sublimate within the environment. The environment containing the sublimate is contacted with a drying agent such as a desiccant to maintain the environment whereby the substance sublimes at substantially atmospheric pressure and at the controlled temperature.
1. A method for continuous lyophilization by sublimation of water in a solid phase within a material, the method comprising:
freezing a material containing water to a temperature below 32° F., whereby the water is present in a solid phase;
continuously supplying the frozen material in particulate form to an inlet of a processing apparatus having a processing chamber containing an air environment;
rotating a plurality of spaced apart trays arranged within the processing chamber;
continuously cascading the frozen material in particulate form received from the inlet downwardly within the processing chamber between the plurality of rotating spaced apart vertically stacked trays for receiving the frozen material within the processing chamber, each of the trays forming a processing zone, each of the trays including at least one aperture to allow the material to continuously cascade from one rotating tray to an adjacent underlying rotating tray;
wherein the cascading comprises continuously discharging the material through the aperture of each rotating tray by engagement of the material with a stationary wiper associated with and overlying each rotating tray;
maintaining a substantially atmospheric air environment in the range of ±0.10 inches water within each of the processing zones and at a temperature in the range of 20−30° F., whereby the water in a solid phase sublimes forming a sublimate including water vapor within the environment;
circulating the environment within the processing chamber by a plurality of fans within the processing chamber;
cooling an exhaust gas from the processing chamber containing the sublimate to form a cooled exhaust gas;
controlling the partial pressure of the water within the environment at each of the processing zones less than the vapor pressure of the water in solid phase in the frozen material by at least contacting the cooled exhaust gas from the processing chamber containing the sublimate with one of a plurality of desiccant systems each containing a desiccant, wherein the plurality of desiccant systems are arranged in parallel with the cooled exhaust gas, wherein the desiccant is selected from the group consisting of lithium chloride, calcium chloride, calcium sulfate, phosphorous pentoxide, triethylene glycol, diethylene glycol, ethylene glycol; tetrathylene glycol, silica gel, and molecular sieves;
controlling the flow of the cooled exhaust gas to one of the plurality of desiccant systems;
heating the cooled exhaust gas after contacting the cooled exhaust gas with one of the desiccant systems to provide a heated exhaust gas;
recycling the heated exhaust gas to the processing chamber;
rejuvenating the desiccant by recovering the sublimate in the form of liquid water to enable reuse of the desiccant in the method; and
reusing in the method the water from the sublimate recovered from the desiccant.
2. The method of claim 1 , wherein cooling the exhaust gas further including condensing the sublimate from the environment.